CN104007188A - Method for detecting illegal cooking oil by using gas chromatograph - Google Patents
Method for detecting illegal cooking oil by using gas chromatograph Download PDFInfo
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- CN104007188A CN104007188A CN201310396440.9A CN201310396440A CN104007188A CN 104007188 A CN104007188 A CN 104007188A CN 201310396440 A CN201310396440 A CN 201310396440A CN 104007188 A CN104007188 A CN 104007188A
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- methanol solution
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Abstract
The invention provides a method for detecting illegal cooking oil by using gas chromatograph. The method comprises the following steps of firstly adding sulfuric an acid-methanol solution or potassium hydroxide-methanol solution in a container with a to-be-detected sample; heating to a temperature of 50-100 DEG C in water bath; keeping the temperature for 30-60 min; adding a boron trifluoride-methanol solution into the container; boiling for 1-5 min; stopping heating and cooling to a room temperature; adding n-hexane into the container; vibrating thoroughly; standing; taking supernatant after the solution is layered; filtering with a filter membrane; collecting filtrate, the filtrate being to-be-detected sample for chromatograph; detecting the filtrate by using the gas chromatograph to generate a chromatogram map; analyzing the chromatogram map; and determining whether the to-be-detected sample is the illegal cooking oil or not. The method for detecting and analyzing the illegal cooking oil by using the gas chromatograph overcomes the disadvantages in the prior art, can detect and identify whether the sample is the illegal cooking oil or not rapidly and accurately.
Description
Technical field
The present invention relates to waste oil detection technique field, particularly related to a kind of method that detects waste oil with gas chromatograph.
Background technology
Waste oil, from the waste grease of catering trade, is the rubbish that municipal sewage system trickles silently.There are some lawless persons to reclaim processing to it, make it transform into " edible oil " on dining table.The paste that these lawless persons fish for a large amount of dim muddinesses every day, slightly take on a red color from Urban Underground water channel, only through manufacturing procedures such as the filtration at a night, heating, precipitation, separation, just can allow these rubbish variable bodies of distributing stench be refrigerant " edible oil ", finally by low price, sell, return to people's dining table.The three-without-product of this being called as " waste oil ", its principal ingredient remains triglyceride, but than real qualified edible oil many cause a disease in a large number, carcinogenic toxicant.Waste oil quality extreme difference, extremely unhygienic, will destroy people's white blood cell and alimentary canal mucous membrane and cause the serious consequences such as food poisoning is even carcinogenic, so waste oil is forbidden for edible oil field by people after being eaten.
While buying edible vegetable oil, consumer generally can be proposed and adopt sense organ means to differentiate.Rule of thumb, edible vegetable oil generally can be by seeing, hear, taste, listen, ask that five aspects differentiate.But for the waste oil inferior doped with objectionable impurities, simply by virtue of people's the sense organ of seeing, hear, taste, listening, differentiate it is very difficult.
At present, the domestic unified standard that not yet has detection waste oil, in existing state compulsory standard < < edible vegetable oil hygienic standard > > (2716-2005), about the physical and chemical index of edible oil, detect comprise that acid value, peroxide value, leaching oil solvent are residual, free phenol (cottonseed oil), total arsenic, lead, aflatoxin, benzopyrene, residues of pesticides totally 9 indexs, respectively plant crude oil and vegetable edible oil are carried out to different standard detection.But plant crude oil, vegetable edible oil are not all waste oils, and even these 9 basic edible oils detect index waste oils to produce the oil coming may be all also qualified in standard, so edible vegetable oil hygienic standard cannot be distinguished detection for waste oil at all.Because the waste oil comparison of ingredients of high acid value is complicated, the specificity physical and chemical index of its detection, also in the experiment investigation stage, accurate qualitative, quantitative still more difficult at present.
Summary of the invention
The invention provides a kind of method of utilizing gas chromatograph that waste oil is detected, analyzed, the method has solved the deficiency in background technology, can be fast, accurately detection and identification whether go out sample be waste oil.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of method that detects waste oil with gas chromatograph, comprise the following steps: (1), in filling the container of detected sample, add sulfuric acid-methanol solution or potassium hydroxide-methanol solution, heating water bath to 50～100 ℃ are also incubated 30～60min at this temperature, the sulfuric acid-methanol solution adding or the volume of potassium hydroxide-methanol solution are sample volume 14～30 times;
(2), in container, add 14～30 times that boron trifluoride methanol solution, the volume adding are sample volume, boil 1～5min, stop heating and being cooled to room temperature;
(3), in container, add 3～14 times that normal hexane, the volume adding are sample volume, fully standing after vibration, after layering, get supernatant membrane filtration, and collect filtrate, filtrate being treated chromatogram detection sample;
(4), filtrate is detected and is generated chromatogram with gas chromatograph, wherein detecting device is fid detector, detector temperature is 250～300 ℃, injector temperature is 200～250 ℃, carrier gas is nitrogen, and flow rate of carrier gas is 1～1.5ml/min, and split ratio is 30～35:1, heating schedule for being warming up to 140 ℃ and stop 5min with the speed of 5 ℃/min at 80 ℃, and then the speed with 2.5 ℃/min is warming up to 230 ℃;
(5), chromatogram is analyzed, judge whether detected sample is waste oil.
In step (5), determine whether that the method for waste oil is as follows: in observation chromatogram, whether occurred that an above retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, if so, sample is waste oil.
In sulfuric acid-methanol solution in step (1), the mass percent of sulfuric acid is 1%～5%, and wherein sulfuric acid is for analyzing the concentrated sulphuric acid that pure concentration is 95～98%, the absolute methanol that described methyl alcohol is greater than 99.5% for analyzing pure concentration.
In potassium hydroxide-methanol solution in step (1), the concentration of potassium hydroxide is 0.1～0.5mol/L, and described potassium hydroxide is for analyzing the potassium hydroxide of purity >=85%.
Boron trifluoride methanol solution in step (2) is for analyzing the boron trifluoride methanol solution that pure concentration is 14～50%.
Described detected sample is for removing after filtration the sample of solid particle residue.
Described gas chromatograph is the HP-5 chromatographic column that U.S. Agilent company produces.
Detection method provided by the present invention, it detects principle: waste oil is that lawless person reclaims by the greasy floating thing in sewer or by the leftovers of hotel, restaurant, leftovers (common name swill), the oil of processing, extracting through operations such as filtration, heating, precipitation, separation, decolouring, washing oil.Commercially available edible vegetable oil all contains the unsaturated fatty acids such as linoleic acid to some extent, when heating is used, the contour warm chemical reaction of linoleic acid generation thermal decomposition in grease, thermal polymerization generates and a series ofly comprises 9,15-octadecadienoic acid, 6,9,12-octatecatrienoic acid, 6,9, the novel substances such as 11-octatecatrienoic acid.9,15-octadecadienoic acid, 18:3(6,9,12), 6, under the gas chromatograph chromatographic condition that 9,11-octatecatrienoic acid builds in this law, on chromatogram, corresponding retention time is respectively: 43.8～44.2min, 47.1～47.5min, 48.5～48.9min.The novel substance of these generations can not exist in natural edible oil, and in the subtractive process of waste oil, be difficult to remove, therefore, select retention time in sample gas chromatogram be the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min as the specific index of differentiating waste oil, specificity is strong.
The present invention includes the configuration of sulfuric acid-methanol solution, the preparation of potassium hydroxide-methanol solution, sample preparation, the structure of gas chromatograph chromatographic condition, the steps such as sample determination and result judgement, the retention time in sample gas chromatogram of take is 43.8～44.2min, 47.1～47.5min, the specific index that the peak that 48.5～48.9min is corresponding is discriminating waste oil, utilizing gas chromatograph is main testing tool, by repetition test, construct complete testing conditions, the present invention can be quick, accurately whether be waste oil to detection and identification if going out sample, detect and be limited to 20 μ g/ml, made up existing national standard defect.
Accompanying drawing explanation
Fig. 1 is blank gas chromatography collection of illustrative plates;
Fig. 2 is the gas chromatography collection of illustrative plates of the peanut oil that detects in embodiment 1;
Fig. 3 is the gas chromatography collection of illustrative plates of the rapeseed oil that detects in embodiment 1;
Fig. 4 is the gas chromatography collection of illustrative plates of the rice oil that detects in embodiment 1;
Fig. 5 is the gas chromatography collection of illustrative plates of the soybean oil that detects in embodiment 2;
Fig. 6 is the gas chromatography collection of illustrative plates of the sunflower oil that detects in embodiment 2;
Fig. 7 is the gas chromatography collection of illustrative plates of the corn oil that detects in embodiment 2;
Fig. 8 is the waste oil gas chromatography collection of illustrative plates detecting in embodiment 3;
Fig. 9 is the waste oil gas chromatography collection of illustrative plates detecting in embodiment 4.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the present invention is done to detailed specific description, the following stated only, in order to be that those skilled in the art understand the cited several specific embodiments of the present invention, is not used for limiting the present invention's scope required for protection.The equivalence of being done with the feature described in the claims in the present invention, structure and principle therefore all changes or modifies, within all should being included in the claims in the present invention scope.
In following examples provided by the present invention, sulfuric acid is for analyzing the concentrated sulphuric acid that pure concentration is 95～98%, the absolute methanol that methyl alcohol is greater than 99.5% for analyzing pure concentration.Described potassium hydroxide is for analyzing the potassium hydroxide of purity >=85%.Boron trifluoride methanol solution is for analyzing the boron trifluoride methanol solution that pure concentration is 14～50%.In following examples, do not do tired stating.
Embodiment 1
Detection method step in the present embodiment is as follows:
The configuration of reagent:
Sulfuric acid-methanol solution: measure sulfuric acid 1ml and add methyl alcohol and be diluted to 100ml, shaking up and being mixed with concentration is sulfuric acid-methanol solution of 1%;
Sample preparation:
First get peanut oil 0.35ml, add sulfuric acid-methanol solution 5ml, 50 ℃ of heating water bath 30min, adding concentration is 15% boron trifluoride methanol solution 5ml, boil 1min, stop heating, be cooled to room temperature, add normal hexane 1ml, vibration, standing, after layering, get 0.45 μ m membrane filtration for supernatant, collect filtrate, obtain testing sample;
Filtrate is detected and is made chromatogram with gas chromatograph, being wherein configured to of gas chromatograph chromatographic condition:
Chromatographic column: HP-5(30m * 0.320mm * 0.25 μ m) U.S. Agilent company,
Detecting device: FID,
Detector temperature: 250 ℃,
Injector temperature: 200 ℃,
Carrier gas: 99.999% nitrogen,
Flow rate of carrier gas: 1ml/min,
Split ratio: 30:1,
Sample size: 1 μ l,
Temperature programme: 80 ℃ → 140 ℃ (5 ℃/min, stop 5min) → 230 ℃ (2.5 ℃/min);
Sample determination and result judgement:
Under the chromatographic condition building, precision measures testing sample 1 μ l, and inject gas chromatograph records the retention time at each peak of chromatogram;
As occurred in testing sample chromatogram, one or more retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, illustrate that testing sample contains 9,15-octadecadienoic acid, 6,9,12-octatecatrienoic acid, 6, one or more materials in 9,11-octatecatrienoic acid, judge that testing sample is waste oil.
In the present embodiment, measured chromatogram as shown in Figure 2, for convenient contrast, has also recorded blank gas chromatogram in the present embodiment, and as shown in Figure 1, what retention time was about 0～2.65min is solvent peak;
In Fig. 2, do not occur that retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, so the testing result in the present embodiment is non-waste oil, testing result is consistent with actual conditions (peanut oil).
In the present embodiment, also adopting uses the same method detects rapeseed oil and rice oil, its testing result respectively as shown in Figure 3 and Figure 4, in Fig. 3 and Fig. 4, do not occur that retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, its testing result is consistent with actual conditions.
Embodiment 2
Detection method step in the present embodiment is as follows:
The configuration of reagent:
Potassium hydroxide-methanol solution: take potassium hydroxide 0.56g and add the dissolving of 100ml methyl alcohol, shake up the potassium hydroxide-methanol solution that is mixed with 0.1mol/L;
Sample preparation:
First get soybean oil 0.35ml, add potassium hydroxide-methanol solution 5ml, 50 ℃ of heating water bath 30min, adding concentration is 25% boron trifluoride methanol solution 5ml, boil 1min, stop heating, be cooled to room temperature, add normal hexane 1ml, vibration, standing, after layering, get 0.45 μ m membrane filtration for supernatant, collect filtrate, obtain testing sample;
Filtrate is detected and is made chromatogram with gas chromatograph, being wherein configured to of gas chromatograph chromatographic condition:
Chromatographic column: HP-5(30m * 0.320mm * 0.25 μ m) U.S. Agilent company,
Detecting device: FID,
Detector temperature: 250 ℃,
Injector temperature: 200 ℃,
Carrier gas: 99.999% nitrogen,
Flow rate of carrier gas: 1ml/min,
Split ratio: 30:1,
Sample size: 1 μ l,
Temperature programme: 80 ℃ → 140 ℃ (5 ℃/min, stop 5min) → 230 ℃ (2.5 ℃/min);
Sample determination and result judgement:
Under the chromatographic condition building, precision measures testing sample 1 μ l, and inject gas chromatograph records the retention time at each peak of chromatogram;
As occurred in testing sample chromatogram, one or more retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, illustrate that testing sample contains 9,15-octadecadienoic acid, 6,9,12-octatecatrienoic acid, 6, one or more materials in 9,11-octatecatrienoic acid, judge that testing sample is waste oil.
In the present embodiment, measured chromatogram as shown in Figure 3, in Fig. 3, do not occur that retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, so the testing result in the present embodiment is non-waste oil, testing result is consistent with actual conditions (soybean oil).
In the present embodiment, also adopting uses the same method detects sunflower oil and corn oil, its testing result respectively as shown in Figure 6 and Figure 7, in Fig. 6 and Fig. 7, do not occur that retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, its testing result is consistent with actual conditions.
Embodiment 3
Detection method step in the present embodiment is as follows:
The configuration of reagent:
Sulfuric acid-methanol solution: measure sulfuric acid 5ml and add methyl alcohol and be diluted to 100ml, shaking up and being mixed with concentration is sulfuric acid-methanol solution of 5%;
Sample preparation:
Learn from else's experience and remove by filter the waste oil 0.35ml of particle residue, add sulfuric acid-methanol solution 10ml, 100 ℃ of heating water bath 60min, adding concentration is 35% boron trifluoride methanol solution 10ml, boil 5min, stop heating, be cooled to room temperature, add normal hexane 5ml, vibration, standing, after layering, get 0.45 μ m membrane filtration for supernatant, collect filtrate, obtain testing sample;
Filtrate is detected and is made chromatogram with gas chromatograph, being wherein configured to of gas chromatograph chromatographic condition:
Chromatographic column: HP-5(30m * 0.320mm * 0.25 μ m) U.S. Agilent company,
Detecting device: FID,
Detector temperature: 300 ℃,
Injector temperature: 250 ℃,
Carrier gas: 99.999% nitrogen,
Flow rate of carrier gas: 1.5ml/min,
Split ratio: 35:1,
Sample size: 1 μ l,
Temperature programme: 80 ℃ → 140 ℃ (5 ℃/min, stop 5min) → 230 ℃ (2.5 ℃/min);
Sample determination and result judgement:
Under the chromatographic condition building, precision measures testing sample 1 μ l, and inject gas chromatograph records the retention time at each peak of chromatogram;
As occurred in testing sample chromatogram, one or more retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, illustrate that testing sample contains 9,15-octadecadienoic acid, 6,9,12-octatecatrienoic acid, 6, one or more materials in 9,11-octatecatrienoic acid, judge that testing sample is waste oil.
In the present embodiment, measured chromatogram as shown in Figure 4, in Fig. 4, occurred that 44.098min, two of 48.741min are included in respectively 9 in 43.8～44.2min, 48.5～48.9min, 15-octadecadienoic acid and 6,9, the characteristic peak of 11-octatecatrienoic acid, therefore judges that it is waste oil, conforms to real conditions.
Embodiment 4
Detection method step in the present embodiment is as follows:
The configuration of reagent:
Potassium hydroxide-methanol solution: take potassium hydroxide 1.4g and add the dissolving of 100ml methyl alcohol, shake up and be mixed with potassium hydroxide-methanol solution that concentration is 0.25mol/L;
Sample preparation:
Learn from else's experience and remove by filter the waste oil 0.35ml of particle residue, add potassium hydroxide-methanol solution 7ml, 80 ℃ of heating water bath 450min, adding concentration is 45% boron trifluoride methanol solution 8ml, boil 3min, stop heating, be cooled to room temperature, add normal hexane 3ml, vibration, standing, after layering, get 0.45 μ m membrane filtration for supernatant, collect filtrate, obtain testing sample;
Filtrate is detected and is made chromatogram with gas chromatograph, being wherein configured to of gas chromatograph chromatographic condition:
Chromatographic column: HP-5(30m * 0.320mm * 0.25 μ m) U.S. Agilent company,
Detecting device: FID,
Detector temperature: 280 ℃,
Injector temperature: 230 ℃,
Carrier gas: 99.999% nitrogen,
Flow rate of carrier gas: 1.3ml/min,
Split ratio: 33:1,
Sample size: 1 μ l,
Temperature programme: 80 ℃ → 140 ℃ (5 ℃/min, stop 5min) → 230 ℃ (2.5 ℃/min);
Sample determination and result judgement:
Under the chromatographic condition building, precision measures testing sample 1 μ l, and inject gas chromatograph records the retention time at each peak of chromatogram;
As occurred in testing sample chromatogram, one or more retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, illustrate that testing sample contains 9,15-octadecadienoic acid, 6,9,12-octatecatrienoic acid, 6, one or more materials in 9,11-octatecatrienoic acid, judge that testing sample is waste oil.
In the present embodiment, measured chromatogram as shown in Figure 5, in Fig. 5, occurred that 44.1min, 47.277min, 47.369min, tetra-of 48.719min are included in respectively 9 in 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, 15-octadecadienoic acid, 18:3(6,9,12) and 6,9, the characteristic peak of 11-octatecatrienoic acid, therefore judges that it is waste oil, conforms to truth.
Claims (7)
1. a method that detects waste oil with gas chromatograph, it is characterized in that comprising the following steps: (1), in filling the container of detected sample, add sulfuric acid-methanol solution or potassium hydroxide-methanol solution, heating water bath to 50～100 ℃ are also incubated 30～60min at this temperature, the sulfuric acid-methanol solution adding or the volume of potassium hydroxide-methanol solution are sample volume 14～30 times;
(2), in container, add 14～30 times that boron trifluoride methanol solution, the volume adding are sample volume, boil 1～5min, stop heating and being cooled to room temperature;
(3), in container, add 3～14 times that normal hexane, the volume adding are sample volume, fully standing after vibration, after layering, get supernatant membrane filtration, and collect filtrate, filtrate being treated chromatogram detection sample;
(4), filtrate is detected and is generated chromatogram with gas chromatograph, wherein detecting device is fid detector, detector temperature is 250～300 ℃, injector temperature is 200～250 ℃, carrier gas is nitrogen, and flow rate of carrier gas is 1～1.5ml/min, and split ratio is 30～35:1, heating schedule for being warming up to 140 ℃ and stop 5min with the speed of 5 ℃/min at 80 ℃, and then the speed with 2.5 ℃/min is warming up to 230 ℃;
(5), chromatogram is analyzed, judge whether detected sample is waste oil.
2. the method that detects waste oil with gas chromatograph according to claim 1, it is characterized in that: in step (5), determine whether that the method for waste oil is as follows: in observation chromatogram, whether occurred that more than one retention time is the peak of 43.8～44.2min, 47.1～47.5min, 48.5～48.9min, if so, sample is waste oil.
3. the method that detects waste oil with gas chromatograph according to claim 1, it is characterized in that: in the sulfuric acid-methanol solution in step (1), the mass percent of sulfuric acid is 1%～5%, wherein sulfuric acid is for analyzing the concentrated sulphuric acid of pure concentration 95～98%, the absolute methanol that described methyl alcohol is greater than 99.5% for analyzing pure concentration.
4. the method that detects waste oil with gas chromatograph according to claim 1, it is characterized in that: in the potassium hydroxide-methanol solution in step (1), the concentration of potassium hydroxide is 0.1～0.5mol/L, described potassium hydroxide is for analyzing the potassium hydroxide of purity >=85%.
5. the method that detects waste oil with gas chromatograph according to claim 1, is characterized in that: the boron trifluoride methanol solution in step (2) is for analyzing the boron trifluoride methanol solution that pure concentration is 14～50%.
6. the method that detects waste oil with gas chromatograph according to claim 1, is characterized in that: described detected sample is for removing after filtration the sample of solid particle residue.
7. the method that detects waste oil with gas chromatograph according to claim 1, is characterized in that: described gas chromatograph is the HP-5 chromatographic column that U.S. Agilent company produces.
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| CN104483342A (en) * | 2014-12-13 | 2015-04-01 | 广西科技大学 | Method for qualitatively detecting hogwash oil |
| CN106370655A (en) * | 2016-08-17 | 2017-02-01 | 安徽省怀远县鑫泰粮油有限公司 | Recovered oil rapid detection method |
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| JP2006200907A (en) * | 2005-01-18 | 2006-08-03 | Eco Up:Kk | Analyzing method of pcb in waste oil |
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| CN104483342A (en) * | 2014-12-13 | 2015-04-01 | 广西科技大学 | Method for qualitatively detecting hogwash oil |
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| CN106370655A (en) * | 2016-08-17 | 2017-02-01 | 安徽省怀远县鑫泰粮油有限公司 | Recovered oil rapid detection method |
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